超高效液相色谱-串联质谱法测定动物源性食品中32种神经系统药物

Determination of 32 kinds of nervous system drugs in animal-derived foods by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法同时检测动物源性食品中32种神经系统药物的方法。方法样品经β-葡萄糖醛酸酶/芳香基硫酸酯酶酶解,酸性乙腈提取,PRiME HLB净化,采用乙腈+0.1%甲酸水作为流动相,超高效液相色谱-串联质谱法确证检测,外标法定量。结果β受体激动剂类药物的检出限为0.2μg/kg;兴奋剂、镇静剂类药物的检出限为0.5μg/kg;麻醉剂类药物的检出限为1.0μg/kg。肌肉基质中32种药物的线性关系良好,相关系数均大于等于0.9916,回收率为61%~106%,相对标准偏差为1.5%~8.7%;肝脏基质中32种药物的线性关系良好相关系数均大于等于0.9914,回收率为60%~110%,相对标准偏差为1.3%~9.6%。结论本方法具有检测药物种类多,检出限低,稳定性好,简便快捷,节省试剂等优势,适用于动物源性食品中多种神经系统药物的检测。

Objective To establish a method for simultaneous determination of 32 kinds of nervous system drugs in the animal-derived foods of livestock and poultry by ultra performance liquid chromatography tandem mass spectrometry.Methods The samples were enzymolized byβ-glucuronidase/aryl sulfatase,extracted by acid acetonitrile,purified by PRiME HLB,confirmed by ultra performance liquid chromatography-tandem mass spectrometry using cetonitrile+0.1%formic acid water as mobile phase,and quantified by external standard method.Results The limit of detection ofβ-agonists was 0.2μg/kg;the limit of detection of stimulants and sedatives was 0.5μg/kg;the limit of detection of anesthetics was 1.0μg/kg.The linear relationships between 32 kinds of drugs in the muscle matrix were good,with correlation coefficients all greater than or equal to 0.9916,and the recovery rates were 61%-106%with relative standard deviations of 1.5%-8.7%.The linear relationships between 32 kinds of drugs in the liver matrix were all greater than or equal to 0.9914,the recovery rates were 60%-110%with the relative standard deviations of 1.3%-9.6%.Conclusion This method has the advantages of detecting a variety of drugs,low limit of detection,good stability,simplicity,speed,and saving reagents,and is suitable for the detection of a variety of nervous system drugs in animal-derived food.